CN102095672A - Multi-method combined particle size analyzer - Google Patents
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Abstract
The invention discloses a multi-method combined particle size analyzer which is characterized in that a laser source, a non-monochromatic lighting source, a microobjective, a Dove prism or two 90-degree turning prisms or total reflection mirrors, a half transparent and half reflecting mirror, an array digital camera or a video camera, a sample cell and a lens form two light path structures, wherein one light path irradiates samples in the sample cell from the non-monochromatic lighting source, and an image magnified by the microobjective is transmitted to the array digital camera through the Dove prism and the half transparent and half reflecting mirror; and the other light path irradiates the samples in the sample cell from the laser lighting source, and the image magnified by the lens is transmitted to the array digital camera through the half transparent and half reflecting mirror. The multi-method combined particle size analyzer has the benefits of combining multiple measuring methods together by using one digital camera, expanding the upper limit and the lower limit of the particle size analyzer by using a simple structure, enabling the measurement range of the particle size analyzer to be from nanometer to hundreds of microns, meeting the requirement of wide-range size distribution measurement, and being capable of giving morphology parameters of particles by using the image method simultaneously.
Description
Technical field
The present invention relates to the grain graininess measurement mechanism of a kind of fused images method and light scattering method, the grain graininess instrument that particularly a kind of measurement range can be from nanometer, sub-micron to micron.
Background technology
With the development of CCD and cmos digital camera, the image method grain graininess analyser that adopts digital camera to replace the eyepiece on the conventional microscope to constitute is used widely in recent years.Be subjected to the restriction of optical microscope theoretical image resolution, the measurement lower limit of image method grain graininess instrument is generally more than 0.5 micron, and the upper limit can be determined according to the enlargement ratio of the microcobjective that uses.Dynamic light scattering grain graininess instrument is mainly used in the granulometry of nano particle, and the general measure lower limit is about 1 nanometer, and the upper limit is at the 3-5 micron.Though these 2 kinds of grain graininess instrument can satisfy the particle sizing in particle size range separately, to tens of during to hundreds of microns, 2 just can't meet the demands the particle size range of measuring particle at needs from nanometer.Static light scattering grain graininess instrument then is a scattered light intensity of measuring a large amount of particles, do not consider that particle does the pulsation of the scattered light intensity that Brownian movement causes, become the main method of present particle sizing based on the grain graininess instrument of static light scattering principle, measurement range can be from sub-micron to hundreds of microns.
Conventional images method grain graininess instrument is to improve on microscope, with original eyepiece on CCD or cmos digital camera or the alternative microscope of digital camera, particulate samples is placed on the microslide, digital camera or digital camera photograph to be delivered to computing machine with output signal behind the micro-image of particle and handles, obtain the image of particle, further obtain the size-grade distribution of particle, parameters such as shape with the grain graininess analysis software.When measuring different size particles, can use the object lens of different enlargement ratios with the rotary object lens mechanism on the microscope instead, but that luminous source system is still is same, does not change because of changing object lens.
Dynamic light scattering grain graininess instrument adopts laser to make light source, incide in the liquid (normally water) that contains tested particle, molecule is subjected to the bump of peripheral fluid molecule in liquid, can produce Brownian movement, this Brownian movement at random makes the particle scattered intensity that random pulse also take place, and its ripple frequency is relevant with grain size, the random motion frequency of larger particles is lower, diffusion motion speed is slower, and higher than the random motion frequency of granule, diffusion motion speed is very fast.The diffusion of particle and the relation of granularity can be described with the Stocks-Einstein formula:
In the formula
D t Be coefficient of diffusion,
K B Be the graceful constant of bohr thatch,
TBe absolute temperature,
ηBe viscosity
, RIt is the radius of particle to be measured.
According to theory of Brownian motion,
Constantly the expectation value of the relative origin displacement of particle square is:
Therefore, if can record nano particle in process
Displacement after time just can obtain coefficient of diffusion
D t ,Use formula (1) to obtain tested particle grain size then
dTake continuously fast the Brownian movement image of particle scattered light particle, the random motion of particle under the analytic record just can be obtained the granularity of particle by the Stocks-Einstein formula.But when particle was big, Brownian movement was very little, can't detect, and also just can not measure the granularity of particle more in this way.It in this measuring method the continuous time series signal of measuring the dynamic scattering of particle.
Static light scattering grain graininess instrument adopts laser as light source equally, incides on the tested particle, and particle can produce light scattering, and this scattering can use Mie ' s light scattering theory to describe.Measure the space distribution of particle scattered light, use Mie ' s light scattering theory and inversion algorithm can obtain the granularity of tested particle then.What measure in the method is the static light scattering intensity relevant with grain size, does not relate to the dynamic effects that movement of particles produces the light scattering Strength Changes, so measuring-signal is not a time series signal.
Summary of the invention
The objective of the invention is the image method grain graininess to be measured and light scattering method grain graininess measurement fusion grain graininess measuring technique together in order to provide a kind of, feasible grain graininess instrument measurement range based on this technology can satisfy various measurement requirement from nanometer to hundreds of microns.
Ultimate principle of the present invention: but with face battle array digital camera or video camera with the controlled and continuous coverage function of shutter speed, as CCD or cmos digital camera or digital camera as the detecting sensor part, when image method is measured, with miniature, as light emitting diode, be arranged in the below of sample cell, light source as the transmission beam method image measurement, or be arranged in around the microcobjective, light source as the reflectometry image measurement, face battle array digital camera or camera arrangements on the focal plane of microcobjective, composing images method grain graininess measuring instrument like this.
When dynamic light scattering measurement, as light source, laser beam is arranged lens from sample cell below incident on the sample cell with laser, and the Simulated dynamic scattering light signals of particle receives photographic images by face battle array digital camera or video camera.Can adopt two kinds of modes to write down the dynamic light scattering signal of particle, a kind of is the space distribution image of continuous recording multiframe particle scattered light, and the Brownian movement characteristic of analyzing the dynamic scattering luminous point of particle in these images then obtains the granularity of particle; Another kind is the shutter speed of control figure camera
Make the particle dynamic light scattering point in the two field picture photograph become a trajectory, the track of all the grain optical scattering points in this two field picture is carried out data processing, obtain coefficient of diffusion, obtain the granularity of particle then by formula (1) by formula (2).
When static light scattering is measured, light path arrangement and dynamic light scattering measurement with, but only the static light scattering characteristic of analysing particulates obtains the granularity of particle.
To the focal length of microcobjective and the focal length of lens in the light scattering measurement, aberration when design is considered in parametric synthesis such as aberration, can be combined into one with these two lens.
Based on the foregoing invention principle, technical scheme of the present invention is: the grain graininess instrument that a kind of multi-method merges, it is characterized in that, this grain graininess instrument is by LASER Light Source, the polyenergetic lighting source, microcobjective, turn back prism or completely reflecting mirror of Dove prism or 2 90 degree constitutes the 180 degree light path of turning back, semi-transparent semi-reflecting lens, face battle array digital camera or video camera, sample cell and lens combination are synthesized two light channel structures, one the tunnel is to be mapped to sample the sample cell from the illumination that the polyenergetic lighting source sends, sample cell is positioned on the sightingpiston of microcobjective, and microcobjective arrives face battle array digital camera or video camera behind the process semi-transparent semi-reflecting lens after enlarged image is passed through Dove prism again; Another road is that illumination that LASER Light Source is sent is mapped to the sample in the sample cell, lens with enlarged image through behind the semi-transparent semi-reflecting lens to face battle array digital camera or video camera;
When image method is measured, place the first polyenergetic lighting source under the sample cell luminous, the second polyenergetic lighting source that is arranged in around the microcobjective is not luminous, as the transmission beam method image measurement; Place the first polyenergetic lighting source under the sample cell not luminous, the second polyenergetic lighting source that is arranged in around the microcobjective is luminous as the reflectometry image measurement;
When dynamic light scattering method is measured, the sample particle of the laser beam irradiation that sends by LASER Light Source in the sample cell, the forward direction dynamic scattering light of particle received by lens after semi-transparent semi-reflecting lens to face battle array digital camera or video camera, the dynamic light scattering signal of face battle array digital camera or video camera continuous recording particle, and send into computing machine, theory of Brownian motion and Stocks-Einstein formula according to particle are handled, and obtain the size-grade distribution of particle; Or the shutter speed of control camera
Make on the image photograph because the movement locus line of the scattering luminous point that particle causes because of Brownian movement appears in time exposure, rather than luminous point, send into computing machine then, theory of Brownian motion and Stocks-Einstein formula according to particle are handled, and obtain the size-grade distribution of particle;
When the static light scattering method is measured, the sample particle of the laser beam irradiation that sends by LASER Light Source in the sample cell, the static scattered light of the forward direction of particle received by lens after semi-transparent semi-reflecting lens to face battle array digital camera or video camera, face battle array digital camera or video camera are sent the static scattered signal of the particle that records into computing machine, handle according to Mie ' s light scattering theory, obtain the size-grade distribution of particle.
Described LASER Light Source is made up of first LASER Light Source and second LASER Light Source, and described first LASER Light Source and second LASER Light Source arrange and form an angle that angle, is generally 90 degree and is arranged vertically greater than 0 degree less than 180 degree.
Described lighting source adopts light emitting diode or pea lamp.
Described battle array digital camera is CCD or cmos digital camera.
The invention has the beneficial effects as follows and utilize same senser element-CCD or cmos digital camera that multiple measuring method is merged, enlarged the granulometry bound of particle size analyzer with simple structure, making can be from nanoscale to hundreds of micron order based on the measurement range of particle size analyzer of the present invention, satisfy the wide range of particle size distributions Testing requirement, and can provide the pattern parameter of particle simultaneously with image method.
Description of drawings
Fig. 1 is the embodiment of the invention 1 synoptic diagram;
Fig. 2 is the embodiment of the invention 2 synoptic diagram;
Fig. 3 is two LASER Light Source synoptic diagram in the embodiment of the invention 2;
Fig. 4 is the embodiment of the invention 3 synoptic diagram;
Fig. 5 is the embodiment of the invention 4 synoptic diagram.
Embodiment
The invention will be further described in conjunction with the accompanying drawings.
Embodiment 1:
The grain graininess instrument that a kind of multi-method merges, by shown in Figure 1, this grain graininess instrument is combined into two light channel structures by LASER Light Source 1, first lighting source 2, second lighting source 3, microcobjective 4, Dove prism 5, semi-transparent semi-reflecting lens 6, face battle array digital camera or video camera 7, sample cell 8 and lens 9, one the tunnel is to be mapped to sample the sample cell 8 from the illumination that lighting source 2 sends, sample cell 8 is positioned on the sightingpiston of microcobjective 4, and microcobjective 4 arrives face battle array digital camera or video camera 7 through semi-transparent semi-reflecting lens 6 backs after enlarged image is passed through Dove prism 5 again; Another road is that illumination that LASER Light Source 1 is sent is mapped to the sample in the sample cell 8, lens 9 with enlarged image through semi-transparent semi-reflecting lens 6 back to face battle array digital camera or video cameras 7, face battle array digital camera or video camera 7 become electric signal to send into computing machine image transitions to handle the size-grade distribution that obtains particle.
When measuring with image method, place first lighting source 2 under the sample cell 8 luminous, second lighting source 3 that is arranged in around the microcobjective is not luminous, as the transmission beam method image measurement; Place first lighting source 2 under the sample cell 8 not luminous, second lighting source 3 that is arranged in around the microcobjective is luminous as the reflectometry image measurement; Described first lighting source 2 and second lighting source 3 all adopt light emitting diode or pea lamp, it also can be other light sources, when needs are observed or are measured tested particle surface characteristic and pattern, second lighting source 3 illuminates sample particle from the oblique upper or the top of sample, microcobjective with enlarged image through Dove prism 5 and semi-transparent semi-reflecting lens 6 backs to face battle array digital camera or video cameras 7, face battle array digital camera or video camera 7 become electric signal to send into computing machine image transitions to handle character of surface and the pattern information that obtains particle.
When dynamic light scattering method is measured, the sample particle of the laser beam irradiation that sends by LASER Light Source 1 in the sample cell 8, the forward direction dynamic scattering light of particle is received by lens 9 after semi-transparent semi-reflecting lens 6 arrives face battle array digital camera or video camera 7, the dynamic light scattering signal of face battle array digital camera or video camera 7 continuous recording particles, and send into computing machine, theory of Brownian motion and Stocks-Einstein formula according to particle are handled, and obtain the size-grade distribution of particle; Or the shutter speed of control camera
Make on the image photograph because the movement locus line of the scattering luminous point that particle causes because of Brownian movement appears in time exposure, rather than luminous point, send into computing machine then, theory of Brownian motion and Stocks-Einstein formula according to particle are handled, and obtain the size-grade distribution of particle;
When the static light scattering method is measured, the sample particle of the laser beam irradiation that sends by LASER Light Source 1 in the sample cell 8, the static scattered light of the forward direction of particle is received by lens 9 after semi-transparent semi-reflecting lens 6 arrives face battle array digital camera or video camera 7, face battle array digital camera or video camera 7 are sent the static scattered signal of the particle that records into computing machine, handle according to Mie ' s light scattering theory, obtain the size-grade distribution of particle.
Embodiment 2:
In embodiment 1, static light scattering and dynamic light scattering measurement all be forward scattering light.Because dynamic light scattering is to measure nanoscale to submicron particles, the dynamic scattering light intensity of these molecules is relatively very weak, but the scattered light intensity in all directions is more even, and the environment parasitic light can produce very big noise to the dynamic scattering light of these molecules.And the forward scattering light of micron particles is stronger, the lateral scattering light intensity relatively a little less than, measure the interference be not subject to the environment parasitic light at forward direction.For addressing this problem, embodiment 2 is proposed, by shown in Figure 2.
Different with embodiment 1 is in the present embodiment dynamic light scattering and static light scattering measure and adopt two LASER Light Source respectively: first LASER Light Source 1 and second LASER Light Source 10, by Fig. 2, shown in Figure 3.When dynamic light scattering measurement, the particle of the laser beam irradiation that second LASER Light Source 10 is sent in the sample cell 8, the particle dynamic light scattering clock signal quilt cover battle array digital camera 7 of side direction 90 degree directions is taken record, can avoid the interference of the very strong forward direction parasitic light of laser beam like this, improve the signal to noise ratio (S/N ratio) of dynamic light scattering measurement signal.And the particle of the laser beam irradiation that first LASER Light Source 1 is sent when static light scattering is measured in the sample cell 8, the forward direction static light scattering signal quilt cover battle array digital camera 7 of particle is taken records.Fig. 3 has represented that static light scattering in the present embodiment measures with first LASER Light Source 1 and the dynamic light scattering measurement layout with second LASER Light Source 10, and first LASER Light Source 1 and second LASER Light Source are spent for 10 one-tenth 90 and be arranged vertically.Wherein dynamic light scattering measurement also can be arranged to different angles with second LASER Light Source 10, and second LASER Light Source 10 and first LASER Light Source 1 are arranged to 60 degree angles or 135 degree angle or other angles.
Embodiment 3:
Adopting static light scattering to measure larger particles, during as hundreds of micron particles, the focal length of the lens 9 among the embodiment 1 needs long, and the instrument size of Gou Chenging is longer like this.For reducing the size of instrument, in the present embodiment, the position of the Dove prism among the embodiment 15 is changed, as shown in Figure 4.Image method directly arrives face battle array digital camera or video camera 7 through microcobjective 4 enlarged images in measuring behind semi-transparent semi-reflecting lens 6.After being received by lens 9, dynamic scattering light in the light scattering measurement or static scattered light arrive face battle array digital camera or video camera 7 through passing through semi-transparent semi-reflecting lens 6 behind the Dove prism 5 again.
In the present embodiment also can be as among the embodiment 2 dynamic light scattering measurement and static light scattering measure and adopt 2 LASER Light Source to be arranged at an angle of 90 respectively, to reduce the interference that parasitic light is measured the side direction scattered light.
Embodiment 4:
Adopted Dove prism to change the round of light in the above-described embodiments, but large-sized Dove prism cost is very high, can adopts lower-cost 2 the 90 degree prism 5 of turning back to replace Dove prism to change the round of light, shown in Fig. 5.Spending the prism of turning back for these 2 90 also can replace with 2 completely reflecting mirror.
Three kinds of shared sample cells of measuring method and a face battle array digital camera in the above-described embodiments.The static light scattering method is measured and dynamic light scattering method is measured also shared same set of measuring system, is the measuring method difference, and described battle array digital camera is CCD or cmos digital camera.
Concrete applicating example of the present invention:
When the measurement mechanism of describing in by embodiment 1 carries out the image method measurement of particle, at first just particle is put into sample cell 8, open lighting source 2, particle is imaged on CCD or the CMOS camera 7 after the image under the irradiation of illumination light amplifies through Dove prism 5 and semi-transparent semi-reflecting lens 6 through microcobjective 4, the image size of the particle that statistics CCD or CMOS camera photograph just can be obtained the granule size of particle again by the enlargement factor of the microcobjective of knowing in advance.The size of adding up all particles that photograph obtains the size-grade distribution of particle with regard to particle.Observe the pattern of measuring particle if desired, close lighting source 2, open lighting source 3, just can measure pattern with the light path particle.
When dynamic light scattering measurement, particle is put into sample cell 8, under the irradiation of laser beam 1, because the scattering luminous point of the random motion space distribution that the Brownian movement of particle causes is taken by CCD or CMOS camera 7 behind lens 9 and semi-transparent semi-reflecting lens 6.The time shutter of control camera, as 100ms, this time shutter promptly is in the formula (2)
According to formula (2), particle is during this period because the Brownian movement meeting stays movement locus on the image that camera is taken, and what of luminous point pixel can obtain particle displacement during this period on the image of being taken by camera
rAccording to formula (2) in the known displacement amount
rAfter can obtain the coefficient of diffusion of particle
D t , can obtain the granularity of particle again by formula (1)
RGeneral particle is less than having tangible Brownian movement below 3 microns, and is not obvious greater than 3 microns Brownian movements later on, also just can not utilize the granulometry of this effect measurement particle again.When carrying out the static light scattering measurement, particle in the sample cell 5 can produce scattering under laser incident, according to Mie ' s light scattering theory, the static light scattering space distribution of particle is relevant with grain size, measure the space distribution of particle static light scattering, calculate by Mie ' s theory and inversion algorithm then, can obtain the granularity of particle.Mie ' s light scattering theory and inversion algorithm carry out calculation process and can find in many lists of references, as books such as " the granulometry technology and the application of particle ".
Claims (4)
1. the grain graininess instrument that merges of a multi-method, it is characterized in that, this grain graininess instrument is by LASER Light Source, the polyenergetic lighting source, microcobjective, turn back prism or 2 completely reflecting mirrors of Dove prism or 2 90 degree constitute the 180 degree light path of turning back, semi-transparent semi-reflecting lens, face battle array digital camera or video camera, sample cell and lens combination are synthesized two light channel structures, one the tunnel is to be mapped to sample the sample cell from the illumination that lighting source sends, sample cell is positioned on the sightingpiston of microcobjective, and microcobjective arrives face battle array digital camera or video camera behind the process semi-transparent semi-reflecting lens after enlarged image is passed through Dove prism again; Another road is that illumination that LASER Light Source is sent is mapped to the sample in the sample cell, lens with enlarged image through behind the semi-transparent semi-reflecting lens to face battle array digital camera or video camera;
When image method is measured, place the first polyenergetic lighting source under the sample cell luminous, the second polyenergetic lighting source that is arranged in around the microcobjective is not luminous, as the transmission beam method image measurement; Place the first polyenergetic lighting source under the sample cell not luminous, the second polyenergetic lighting source that is arranged in around the microcobjective is luminous as the reflectometry image measurement;
When dynamic light scattering method is measured, the sample particle of the laser beam irradiation that sends by LASER Light Source in the sample cell, the forward direction dynamic scattering light of particle received by lens after semi-transparent semi-reflecting lens to face battle array digital camera or video camera, the dynamic light scattering signal of face battle array digital camera or video camera continuous recording particle, and send into computing machine, theory of Brownian motion and Stocks-Einstein formula according to particle are handled, and obtain the size-grade distribution of particle; Or the shutter speed of control camera, make on the image photograph because the movement locus line of the scattering luminous point that particle causes because of Brownian movement appears in time exposure, rather than luminous point, send into computing machine then, theory of Brownian motion and Stocks-Einstein formula according to particle are handled, and obtain the size-grade distribution of particle;
When the static light scattering method is measured, the sample particle of the laser beam irradiation that sends by LASER Light Source in the sample cell, the static scattered light of the forward direction of particle received by lens after semi-transparent semi-reflecting lens to face battle array digital camera or video camera, face battle array digital camera or video camera are sent the static scattered signal of the particle that records into computing machine, handle according to Mie ' s light scattering theory, obtain the size-grade distribution of particle.
2. the grain graininess instrument that multi-method according to claim 1 merges, it is characterized in that, described LASER Light Source is made up of first LASER Light Source and second LASER Light Source, and angle becomes less than 180 degree between described first LASER Light Source and second LASER Light Source, arranges greater than 0 degree.
3. the grain graininess instrument that multi-method according to claim 1 merges is characterized in that, described polyenergetic lighting source adopts light emitting diode or pea lamp.
4. the grain graininess instrument that multi-method according to claim 1 merges is characterized in that described battle array digital camera is CCD or cmos digital camera.
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| CN102288523A (en) * | 2011-07-19 | 2011-12-21 | 中国科学技术大学 | Granular grain diameter distribution measuring device based on linear array CCD (charge-coupled device) |
| CN102879318A (en) * | 2012-10-15 | 2013-01-16 | 南京浪博科教仪器研究所 | Nanoparticle measurement device and method |
| CN103954538A (en) * | 2014-05-09 | 2014-07-30 | 河北大学 | Dry-type granule granularity measuring device |
| CN103954537A (en) * | 2014-05-09 | 2014-07-30 | 河北大学 | Dry type particle granularity measuring method |
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| CN102879318A (en) * | 2012-10-15 | 2013-01-16 | 南京浪博科教仪器研究所 | Nanoparticle measurement device and method |
| CN103954538A (en) * | 2014-05-09 | 2014-07-30 | 河北大学 | Dry-type granule granularity measuring device |
| CN103954537A (en) * | 2014-05-09 | 2014-07-30 | 河北大学 | Dry type particle granularity measuring method |
| CN104089858A (en) * | 2014-07-21 | 2014-10-08 | 上海理工大学 | Particle size analyzer |
| CN104359809B (en) * | 2014-10-30 | 2016-12-28 | 顾玉奎 | A kind of compact spiral PM2.5 concentration detection apparatus based on total reflection prism |
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| CN105651661B (en) * | 2016-03-21 | 2018-07-03 | 上海理工大学 | A kind of on-line measurement device and its measuring method for discharging dust concentration and granularity |
| CN105973772A (en) * | 2016-07-01 | 2016-09-28 | 丹东百特仪器有限公司 | Laser granularity measurement instrument with combination of dynamic and static light scattering |
| CN106596354A (en) * | 2016-12-08 | 2017-04-26 | 南京信息工程大学 | Light scattering property measurement device and method based on microlens array |
| CN106596354B (en) * | 2016-12-08 | 2020-03-31 | 南京信息工程大学 | Light scattering characteristic measuring device and method based on micro-lens array |
| CN109141811A (en) * | 2018-08-15 | 2019-01-04 | 中国计量大学 | A kind of particle dynamic trajectory measuring system and method based on asynchronous time expander method |
| CN109724901A (en) * | 2018-12-29 | 2019-05-07 | 中国科学院长春光学精密机械与物理研究所 | A kind of micro particles optical detection apparatus |
| CN109724901B (en) * | 2018-12-29 | 2020-10-13 | 中国科学院长春光学精密机械与物理研究所 | Micron particle optical detection device |
| CN113340894A (en) * | 2021-05-28 | 2021-09-03 | 上海睿钰生物科技有限公司 | Detection method of non-transparent particles |
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